HRID50200
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
11.4 g (63 mmol) of 4-cyanophenoxyacetic acid were dissolved in 200 mL of absolute tetrahydrofuran and mixed at room temperature with 10.2 g (63 mmol) of N,N′-carbonyldiimidazole. After 15 minutes at 60° C., 5.70 g (41.5 mmol) of 2-amino-3-methylamino-6-methylpyridine were added. After 2 hours at 60° C., the solvent was distilled off and the crystalline residue was mixed with water, washed with water, and dried. After crystallization from ethanol, 9.95 g (91% of theory) were obtained in the form of white crystals. C16H14N4O (278.32). Mass spectrum: M+=278.
WORKUP
后处理
- waitAfter 2 hours at 60° C.
- distillationthe solvent was distilled off
- additionthe crystalline residue was mixed with water
- washwashed with water
- customdried
- customAfter crystallization from ethanol
- custom9.95 g (91% of theory) were obtained in the form of white crystals